CN103667768A - Silver target manufacturing method - Google Patents
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- CN103667768A CN103667768A CN201310718028.4A CN201310718028A CN103667768A CN 103667768 A CN103667768 A CN 103667768A CN 201310718028 A CN201310718028 A CN 201310718028A CN 103667768 A CN103667768 A CN 103667768A
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Abstract
The invention relates to the field of target manufacturing and particularly relates to a silver target manufacturing method. The silver target manufacturing method comprises the following steps: selecting a silver raw material with purity of over 4N, fusing the silver raw material by utilizing the atmosphere smelting or vacuum smelting method, casting the melt and then cooling to form an ingot blank; immediately carrying out thermal insulation heat treatment on the ingot blank, i.e., carrying out thermal insulation homogenization within the temperature range of 400 to 900 DEG C and then carrying out hot rolling or forging by an air hammer to form a silver blank, wherein the thermal insulation time is over 0.5h; carrying out cold rolling on the silver blank to form a cold-rolled blank; and carrying out annealing heat treatment on the cold-rolled blank for 0.5 to 3 hours at the annealing heat treatment temperature of 350 to 700 DEG C to obtain a silver target blank with fine and uniform crystal grains and finally, machining by a machine tool to obtain a large-size silver target. The process is higher in machining efficiency and can produce the lower-cost large-size silver target with high quality.
Description
Technical field
The present invention relates to target and manufacture field, relate in particular to a kind of silver-colored target manufacture method.
Background technology
Physical vapor deposition (PVD, Physical Vapor Deposition) be widely used in the high-end manufacturing industry such as optics, electronics, information, the target using in PVD is one of most important starting material in the manufacturing processedes such as liquid-crystal display, solar cell, unicircuit.
Because of argent, there is the premium propertiess such as low resistance and high-reflectivity, and by a large amount of thin layers for the production of electrode or reflecting layer, in the products such as optical record medium, solar cell, low emissivity glass, liquid-crystal display, silver thin layer is raw material mainly with silver-colored target greatly, adopts sputter coating mode to form.
The silver-colored target of industrial application need possess following characteristic:
1, homogeneous microstructure, subsurface defect (slag inclusion, pore, crackle etc.) is few, even zero defect;
2, crystal grain is tiny evenly;
3, purity is high, and foreign matter content is few.
Development along with large-size glass plated film industries such as liquid-crystal display, solar cells, the product sizes such as one side indicating meter, solar cell continue to increase, on the other hand for improving plated film efficiency and reducing costs, cause sizes of substrate increasing, target size also increases thereupon, therefore require also more and more higher to the manufacture of target.In general, in industry, the mode of conventional multi-disc target splicing is used large-size target, but the sheet number of splicing is more, splicing gap is also many, at coating process, can affect plasma body uniformity consistency, and may cause local undesired electric discharge, thereby can reduce quality and the yield of coated product, in addition, splicing quantity is more, quality consistency between each sheet is more difficult consistent, finally also can reduce homogeneity and the product quality of rete.
During as low emissivity glass plated film, target total length can reach 3750mm, and the monolithic size of splicing can reach 600mm, and has the trend that increases gradually monolithic maximum length; And in thin-film solar cells industry, the length 1410mm of common plated film target, it is generally the three-chip type connecting method of the thick intermediate thin in two ends, the middle nearly 1000mm of monolithic splicing length; The circular silver-colored target of small size that conventional optical disc industry is used is produced by forging mode, but because forging equipment investment is large, cost is high, and is subject to the restriction of forging mold size, and the target size of manufacture is compared with little and be difficult to amplify; Therefore the forging mode of the former silver of the small size for CD industry target has been difficult to meet the need of production of current large size product.
Summary of the invention
A kind of manufacture method that can produce large size, high-quality, low-cost silver-colored target in batches that the object of the invention is to overcome deficiency of the prior art and provide.
A kind of silver-colored target manufacture method of the present invention, comprises the steps:
Step (1): select the above silver material of purity 4N, utilize the method for melting in air or vacuum melting by silver material melting, and will melt soup casting, the molten soup naturally cooling after casting forms ingot casting blank.
Step (2): step (1) the formed ingot casting blank of casting is carried out to heat preservation hot processing immediately, 400 ~ 900 ℃ of temperature ranges, be incubated homogenizing, more than soaking time 0.5h, the ingot casting blank after then heat preservation hot being processed carries out that hot rolling is prolonged or air hammer forges, and forms silver-colored base.
Step (3): after step (2) gained silver base cool to room temperature, under the environment of room temperature, silver-colored base is carried out to cold rolling prolonging, form cold rolling base; .
Step (4): the cold rolling formed cold rolling base of step (3) is done to annealing thermal treatment, annealing thermal treatment temp is 350 ~ 700 ℃, time is 0.5 hour ~ 3 hours, obtains the tiny and uniform silver-colored target base of crystal grain, finally by machine tooling, can obtain large size silver target.
Selecting purity is that the state of the above silver material of 4N is silver ingot, silver powder and silver granuel.
The instrument that utilizes the melting of melting in air method to use is atmosphere induction melting furnace.
The instrument that utilizes vacuum smelting method melting to use is vacuum induction melting furnace.
In step (2), the heat treated optimum temps of insulation is 600 ~ 800 ℃.
Hot rolling is prolonged or air hammer forges rolls and prolong than being 30% ~ 70% in step (2), preferably rolls and prolongs than being 40% ~ 60%.
Cold rolling prolonging than being 30% ~ 85% in step (3), wherein cold rolling prolonging than being 50% ~ 70% preferably.
In step (4), the heat treated temperature of annealing is 400 ~ 600 ℃.
Tool of the present invention has the following advantages:
By above-mentioned to high purity silver ingot casting blank carry out heat preservation hot processing and heat preservation hot is processed after ingot casting blank directly carry out that hot rolling is prolonged or air hammer forges, reduced the resistance to deformation of silver ingot, make the coarse grain of as-cast condition broken, remarkable crack healing, reduce or eliminate casting flaw, improved the performance of silver ingot.In addition, after high-purity silver ingot hot rolling being prolonged or air hammer forges, silver-colored base after again hot calender or air hammer being forged carries out cold rolling prolonging, reduce silver-colored base thickness, extend the length of silver-colored base, to obtain required product size, the more important thing is the enough strain energies of the inner acquisition of silver-colored base, finally, by thermal treatment that the cold rolling base after cold rolling is annealed, reach the object of crystal grain thinning and can obtain uniform grain structure in whole silver ingot scope.
For the silver-colored target that only adopts cold-rolling process to produce, in hot rolling, live and prolong in the technique combining with cold rolling, its silver ingot blank can not prolong to press and cracks due to the heat of large deformation, can eliminate casting flaw by the hot rolling of single pass aximal deformation value, have very high working (machining) efficiency simultaneously; Can be because material stress cracks yet, therefore reduced the waste of the material that the generation because of crackle causes; When heat is prolonged silver ingot after pressure and avoided cold rolling, because of work hardening, carry out process annealing repeatedly to remove machining stress, therefore, this technique has higher working (machining) efficiency and can produce the silver-colored target of colory large size.
This silver-colored target manufacture method forges method relatively, and facility investment is low, and has saved forge die expense, therefore, has reduced on the whole the production cost of silver-colored target.
The silver-colored target crystalline grains size that this silver-colored target manufacture method is produced is less than 200 μ m, and even grain-size is more small to 50 μ m, and even grain size, has fine qualities.
Accompanying drawing explanation
Fig. 1 is production scheme of the present invention.
Fig. 2 is the Photomicrograph of the silver-colored target that obtains of application the present invention.
Specific embodiments
By embodiment, further describe the present invention below, but the present invention is not limited only to following embodiment.
Embodiment: the present invention has following flow process as shown in Figure 1.
Step 1: adopt electrolysis silver granuel more than purity 4N, utilize melting in air stove to be heated to approximately 1000 ℃ of meltings, and cooling formation ingot casting blank after casting, ingot casting blank is of a size of 300 mm * 290 mm * 120mm; And by ingot casting blank air cooling to lower than 700 ℃.
Step 2: the ingot casting blank of step 1 gained is placed in to 700 ℃ of heat preservation hot of annealing furnace and processes 1 hour.
Step 3: the ingot casting blank of step 2 is carried out to hot rolling with milling train and prolong, total hot rolling working modulus is 45%;
Before rolling, ingot casting blank is of a size of: length is 300mm, and width is 290mm, and thickness is 120mm, and the silver-colored base after rolling is of a size of: length is 543mm, and width is 291mm, and thickness is 66mm.
Table 1 show the ingot casting blank hot calender that is of a size of 300*290*120mm to the process of 543*291*66mm silver base in calendering amount and the relation of rolling between passage:
| Passage | Height (mm) before calendering | Amount of pressure drop (mm) | Height (mm) after calendering |
| 1 | 120 | 10 | 110 |
| 2 | 110 | 10 | 100 |
| 3 | 100 | 10 | 90 |
| 4 | 90 | 8 | 82 |
| 5 | 82 | 8 | 74 |
| 6 | 74 | 8 | 66 |
Table 1
Step 4: the silver-colored base of step 3 gained is carried out to cold rolling prolonging again with milling train, and the amount of pressure drop of single track processing is 1mm, and total cold rolling rate of prolonging is 51.5%; Cold rolling front silver-colored base is of a size of 543*291*66mm, and cold rolling rear cold rolling base is 1117*292*32mm.
Step 5: the cold rolling formed cold rolling base of step 4 is done to the thermal treatment of finally annealing in annealing furnace, and annealing heat-treat condition is 500 ℃, is incubated 2 hours.
Step 6: the silver-colored target base of step 5 gained is carried out carrying out machining on milling machine, obtain large size, high-quality, low-cost silver-colored target that monolithic is of a size of 1000*280*30mm.
Figure 2 shows that the Photomicrograph of the silver-colored target obtaining according to aforementioned production method, the grain-size of known this silver target is less than 200 μ m, is about 50 μ m.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can utilize method and the technology contents of above-mentioned announcement to make possible change and modification to technical solution of the present invention; therefore; every content that does not depart from technical solution of the present invention; any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all belong to the protection domain of technical solution of the present invention.
Claims (8)
1. a kind of silver-colored target manufacture method of the present invention, is characterized in that: comprise the steps:
Step (1): select the above silver material of purity 4N, utilize the method for melting in air or vacuum melting by silver material melting, and will melt soup casting, the cooling formation ingot casting of the molten soup blank after casting;
Step (2): step (1) the formed ingot casting blank of casting is carried out to heat preservation hot processing immediately, 400 ~ 900 ℃ of temperature ranges, be incubated homogenizing, more than soaking time 0.5h, the ingot casting blank after then heat preservation hot being processed carries out that hot rolling is prolonged or air hammer forges, and forms silver-colored base;
Step (3): after step (2) gained silver base cool to room temperature, under the environment of room temperature, silver-colored base is carried out to cold rolling prolonging, form cold rolling base;
Step (4): the cold rolling formed cold rolling base of step (3) is done to annealing thermal treatment, annealing thermal treatment temp is 350 ~ 700 ℃, time is 0.5 hour ~ 3 hours, obtains the tiny and uniform silver-colored target base of crystal grain, finally by machine tooling, can obtain large size silver target.
2. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: selecting purity is that the state of the above silver material of 4N is silver ingot, silver powder and silver granuel.
3. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: the instrument that utilizes the melting of melting in air method to use is atmosphere induction melting furnace.
4. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: the instrument that utilizes vacuum smelting method melting to use is vacuum induction melting furnace.
5. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: in step (2), the heat treated optimum temps of insulation is 600 ~ 800 ℃.
6. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: in step (2), hot rolling is prolonged or air hammer forges rolls and prolong than being 30% ~ 70%, preferably rolls and prolongs than being 40% ~ 60%.
7. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: cold rolling prolonging than being 30% ~ 85% in step (3), wherein cold rolling prolonging than being 50% ~ 70% preferably.
8. a kind of silver-colored target manufacture method as claimed in claim 1, is characterized in that: in step (4), the heat treated temperature of annealing is 400 ~ 600 ℃.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104651784A (en) * | 2015-03-13 | 2015-05-27 | 福建省诺希科技园发展有限公司 | Manufacturing method of carbon-silver composite target for curved touch screen |
| CN104817277A (en) * | 2015-04-21 | 2015-08-05 | 福建省诺希科技园发展有限公司 | Method for preparing radiation-proof glass by silver composite target and product |
| CN106893990A (en) * | 2017-02-17 | 2017-06-27 | 南京东锐铂业有限公司 | The production technology of silver-colored sputtering target material component |
| CN107523795A (en) * | 2017-10-24 | 2017-12-29 | 宝鸡市铭坤有色金属有限公司 | A kind of manufacture method of titanium target material |
| CN109082637A (en) * | 2018-08-15 | 2018-12-25 | 四川省有色冶金研究院有限公司 | A kind of high uniformly fine grain tin target and preparation method thereof of high-purity |
| CN110643959A (en) * | 2019-10-28 | 2020-01-03 | 冯波 | Method for manufacturing magnesium target material |
| CN111962030A (en) * | 2020-06-29 | 2020-11-20 | 昆山嘉美荣材料科技有限公司 | Manufacturing method of rotary silver target |
| CN113106362A (en) * | 2021-03-18 | 2021-07-13 | 先导薄膜材料（广东）有限公司 | Manufacturing method of target material back plate with concave surface |
| CN113444914A (en) * | 2021-07-19 | 2021-09-28 | 福建阿石创新材料股份有限公司 | Silver-based alloy and preparation method thereof, silver alloy composite film and application thereof |
| CN114196926A (en) * | 2021-11-19 | 2022-03-18 | 有研亿金新材料有限公司 | Short-process high-efficiency preparation method of high-purity copper and copper alloy sputtering target material |
| CN114890689A (en) * | 2022-05-06 | 2022-08-12 | 浙江聚丰玻璃有限公司 | Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof |
| CN114959271A (en) * | 2022-05-18 | 2022-08-30 | 济源豫金靶材科技有限公司 | Recovery method of sputtering silver residual target material |
| CN115141952A (en) * | 2022-07-05 | 2022-10-04 | 株洲火炬安泰新材料有限公司 | High-purity silver target material and processing method thereof |
| CN115976478A (en) * | 2022-12-13 | 2023-04-18 | 江苏迪纳科精细材料股份有限公司 | Silver sulfide resistant alloy target material and preparation method thereof |
| CN115992342A (en) * | 2022-12-15 | 2023-04-21 | 先导薄膜材料（广东）有限公司 | High-purity silver sputtering target material and preparation method thereof |
| CN116695075A (en) * | 2023-06-28 | 2023-09-05 | 宁波江丰电子材料股份有限公司 | Hafnium target blank and preparation method and application thereof |
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| CN104651784A (en) * | 2015-03-13 | 2015-05-27 | 福建省诺希科技园发展有限公司 | Manufacturing method of carbon-silver composite target for curved touch screen |
| CN104651784B (en) * | 2015-03-13 | 2017-05-17 | 福建省诺希科技园发展有限公司 | Manufacturing method of carbon-silver composite target for curved touch screen |
| CN104817277A (en) * | 2015-04-21 | 2015-08-05 | 福建省诺希科技园发展有限公司 | Method for preparing radiation-proof glass by silver composite target and product |
| CN104817277B (en) * | 2015-04-21 | 2017-04-19 | 福建省诺希科技园发展有限公司 | Method for preparing radiation-proof glass by silver composite target and product |
| CN106893990A (en) * | 2017-02-17 | 2017-06-27 | 南京东锐铂业有限公司 | The production technology of silver-colored sputtering target material component |
| CN106893990B (en) * | 2017-02-17 | 2019-02-01 | 南京东锐铂业有限公司 | The production technology of silver-colored sputtering target material component |
| CN107523795A (en) * | 2017-10-24 | 2017-12-29 | 宝鸡市铭坤有色金属有限公司 | A kind of manufacture method of titanium target material |
| CN109082637A (en) * | 2018-08-15 | 2018-12-25 | 四川省有色冶金研究院有限公司 | A kind of high uniformly fine grain tin target and preparation method thereof of high-purity |
| CN110643959A (en) * | 2019-10-28 | 2020-01-03 | 冯波 | Method for manufacturing magnesium target material |
| CN111962030A (en) * | 2020-06-29 | 2020-11-20 | 昆山嘉美荣材料科技有限公司 | Manufacturing method of rotary silver target |
| CN113106362A (en) * | 2021-03-18 | 2021-07-13 | 先导薄膜材料（广东）有限公司 | Manufacturing method of target material back plate with concave surface |
| CN113444914A (en) * | 2021-07-19 | 2021-09-28 | 福建阿石创新材料股份有限公司 | Silver-based alloy and preparation method thereof, silver alloy composite film and application thereof |
| WO2023001137A1 (en) * | 2021-07-19 | 2023-01-26 | 福建阿石创新材料股份有限公司 | Silver-based alloy, preparation method therefor, silver alloy composite thin film and use thereof |
| CN114196926A (en) * | 2021-11-19 | 2022-03-18 | 有研亿金新材料有限公司 | Short-process high-efficiency preparation method of high-purity copper and copper alloy sputtering target material |
| CN114890689A (en) * | 2022-05-06 | 2022-08-12 | 浙江聚丰玻璃有限公司 | Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof |
| CN114959271A (en) * | 2022-05-18 | 2022-08-30 | 济源豫金靶材科技有限公司 | Recovery method of sputtering silver residual target material |
| CN114959271B (en) * | 2022-05-18 | 2024-01-23 | 济源豫金靶材科技有限公司 | Recovery method of sputtering silver residual target |
| CN115141952A (en) * | 2022-07-05 | 2022-10-04 | 株洲火炬安泰新材料有限公司 | High-purity silver target material and processing method thereof |
| CN115976478A (en) * | 2022-12-13 | 2023-04-18 | 江苏迪纳科精细材料股份有限公司 | Silver sulfide resistant alloy target material and preparation method thereof |
| CN115976478B (en) * | 2022-12-13 | 2023-11-28 | 江苏迪纳科精细材料股份有限公司 | Silver sulfide resistant alloy target and preparation method thereof |
| CN115992342A (en) * | 2022-12-15 | 2023-04-21 | 先导薄膜材料（广东）有限公司 | High-purity silver sputtering target material and preparation method thereof |
| CN115992342B (en) * | 2022-12-15 | 2024-06-07 | 先导薄膜材料（广东）有限公司 | High-purity silver sputtering target material and preparation method thereof |
| CN116695075A (en) * | 2023-06-28 | 2023-09-05 | 宁波江丰电子材料股份有限公司 | Hafnium target blank and preparation method and application thereof |
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Application publication date: 20140326 |